JP2022023018A - METHOD FOR MANUFACTURING Nd-Fe-B BASED SINTERED MAGNETIC MATERIAL - Google Patents
METHOD FOR MANUFACTURING Nd-Fe-B BASED SINTERED MAGNETIC MATERIAL Download PDFInfo
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- 239000000696 magnetic material Substances 0.000 title claims abstract description 83
- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 57
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 title abstract description 23
- 238000009792 diffusion process Methods 0.000 claims abstract description 122
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 40
- 239000000956 alloy Substances 0.000 claims abstract description 40
- 239000000843 powder Substances 0.000 claims abstract description 39
- 239000010949 copper Substances 0.000 claims abstract description 31
- 230000032683 aging Effects 0.000 claims abstract description 14
- 229910052802 copper Inorganic materials 0.000 claims abstract description 14
- 239000000126 substance Substances 0.000 claims abstract description 13
- 229910052692 Dysprosium Inorganic materials 0.000 claims abstract description 9
- 229910052771 Terbium Inorganic materials 0.000 claims abstract description 9
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 8
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 claims abstract description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 5
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical group [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims abstract description 5
- 230000014509 gene expression Effects 0.000 claims abstract description 4
- 238000009826 distribution Methods 0.000 claims description 56
- 239000002245 particle Substances 0.000 claims description 35
- 230000006698 induction Effects 0.000 claims description 11
- 238000010298 pulverizing process Methods 0.000 abstract description 2
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 40
- 229910052761 rare earth metal Inorganic materials 0.000 description 30
- 239000000758 substrate Substances 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 13
- 150000002910 rare earth metals Chemical class 0.000 description 13
- 239000002994 raw material Substances 0.000 description 11
- 238000010438 heat treatment Methods 0.000 description 9
- 230000005389 magnetism Effects 0.000 description 9
- 229910052779 Neodymium Inorganic materials 0.000 description 8
- 229910052796 boron Inorganic materials 0.000 description 8
- 229910052742 iron Inorganic materials 0.000 description 8
- 238000005259 measurement Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 230000007423 decrease Effects 0.000 description 5
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 239000012466 permeate Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 229910052777 Praseodymium Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- -1 rare earth fluoride Chemical class 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 238000000441 X-ray spectroscopy Methods 0.000 description 1
- 229910000808 amorphous metal alloy Inorganic materials 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
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- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0293—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
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- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/147—Alloys characterised by their composition
- H01F1/153—Amorphous metallic alloys, e.g. glassy metals
- H01F1/15341—Preparation processes therefor
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- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/0536—Alloys characterised by their composition containing rare earth metals sintered
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- H—ELECTRICITY
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- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
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- H01F7/00—Magnets
- H01F7/02—Permanent magnets [PM]
- H01F7/0205—Magnetic circuits with PM in general
- H01F7/021—Construction of PM
Abstract
Description
本発明はＮｄ－Ｆｅ－Ｂ系永久磁性体の技術分野に属し、Ｎｄ－Ｆｅ－Ｂ系焼結磁性体の製造方法、特に希土類元素の拡散処理方法に関する。 The present invention belongs to the technical field of Nd-Fe-B-based permanent magnetic material, and relates to a method for producing an Nd-Fe-B-based sintered magnetic material, particularly a method for diffusing rare earth elements.
Ｎｄ－Ｆｅ－Ｂ系磁性体は、現在最も優れた磁性材料として、幅広い分野に応用されている。使用条件の苛烈化と希土類資源使用量の増加に伴い、高性能化及び低コスト化は、Ｎｄ－Ｆｅ－Ｂ系磁性体開発の主要テーマとなっている。 The Nd-Fe-B-based magnetic material is currently applied to a wide range of fields as the most excellent magnetic material. With the fierce usage conditions and the increase in the amount of rare earth resources used, higher performance and lower cost have become the main themes for the development of Nd-Fe-B-based magnetic materials.
低コスト及び高性能という目標を実現するために、微量元素の種類及び添加量の最適化、微粉化プロセス、低酸素プロセス等が業界で広く用いられており、重希土類元素の拡散プロセスは、近年、Ｎｄ－Ｆｅ－Ｂ系焼結磁性体の性能を向上させる重要かつ有効な手段となっている。 In order to achieve the goals of low cost and high performance, optimization of trace element types and addition amounts, pulverization process, low oxygen process, etc. are widely used in the industry, and the diffusion process of heavy rare earth elements has been widely used in recent years. , Nd-Fe-B is an important and effective means for improving the performance of the sintered magnetic material.
現在、最も多く用いられている拡散プロセスは、重希土類フッ化物又は水素化物粉末を埋粉・拡散、又は重希土類合金の有機溶液をコーティング、スプレー等の方法で付着させて拡散させるものである。拡散効果を向上させ、原材料のコストを削減するために、多くの企業や科学研究機関が拡散源及び拡散方法の最適化を追求している。 Currently, the most commonly used diffusion process is to embed and diffuse heavy rare earth fluoride or hydride powder, or to attach and diffuse an organic solution of heavy rare earth alloy by coating, spraying, or the like. Many companies and scientific research institutes are pursuing optimization of diffusion sources and methods in order to improve the diffusion effect and reduce the cost of raw materials.
例えば、中国特許ＣＮ１０５５１３７３４Ｂ公報には、ＲＬｘＲＨｙＭｚシリーズ合金を拡散源として用い、残留磁気と磁気エネルギー積を大きく低下させることなく保磁力を大幅に向上させる技術が開示されている。しかしながら当該技術は、拡散合金を平均粒径２．４ミクロンの粉末にするため、プロセスコストが増加し、且つ、酸素含有量が増加して拡散効果に影響を与える可能性があり、保磁力の向上にはまだ改善の余地がある。 For example, the Chinese patent CN105513734B gazette discloses a technique of using an RL x RH yM z series alloy as a diffusion source to significantly improve the coercive force without significantly reducing the residual magnetism and the magnetic energy product. However, in this technique, since the diffusion alloy is made into a powder having an average particle size of 2.4 microns, the process cost increases and the oxygen content may increase to affect the diffusion effect. There is still room for improvement.
また中国特許ＣＮ１０５３５５３５３Ｂ公報には、Ｎｄ－Ｆｅ－Ｂ系焼結磁性体に対して重希土類アモルファス合金を拡散させる技術が開示されている。これにより、合金拡散磁性体の酸化を減少させ、保磁力を大幅に向上あせているが、純重希土類合金を拡散させることで、拡散深さが制限され、保磁力の更なる向上は困難である。 Further, the Chinese patent CN105355353B gazette discloses a technique for diffusing a heavy rare earth amorphous alloy with an Nd—Fe—B based sintered magnetic material. This reduces the oxidation of the alloy diffusing magnetic material and greatly improves the coercive force. However, by diffusing the pure heavy rare earth alloy, the diffusion depth is limited and it is difficult to further improve the coercive force. be.
また中国特許ＣＮ１０７２５１１７６Ｂ公報には、Ｒ２－Ｇａ－Ｃｕ系合金とＲ１－Ｔ１－Ａ－Ｘ系合金とを接触させた後、低温で熱処理して拡散させることで、低温下で良好な拡散効果を実現する技術が開示されている。しかしながら、当該プロセスに係る二つの合金は、いずれも成分に対する要求が高く、厳格な調整条件も要求される等の問題がある。 Further, according to the Chinese patent CN107251176B publication, the R2 - Ga-Cu alloy and the R1-1 - AX alloy are brought into contact with each other and then heat-treated at a low temperature to diffuse, which is good at a low temperature. A technique for realizing a diffusion effect is disclosed. However, the two alloys involved in this process both have high requirements for components and have problems such as strict adjustment conditions.
このように、重希土類又は重希土類水素化物及びフッ化物を用いて拡散する従来の方法では、拡散面に近い領域に重希土類元素が集中し、拡散面から遠い領域では元素が拡散しないか低濃度となり、交換結合作用を奏することが難しい。同時に、拡散面に近い領域では、拡散した元素の濃度が高いことから、重希土類が主相の結晶粒界に浸透し、残留磁気が大幅に低下してしまう。また重希土類元素の損耗が早くなり、深くなるに伴い、重希土類の濃度が急激に低下し、成分構造が不均一になり、性能向上の妨げとなっている。 As described above, in the conventional method of diffusing using heavy rare earths or heavy rare earth hydrides and fluorides, the heavy rare earth elements are concentrated in the region near the diffusion surface, and the elements do not diffuse or have a low concentration in the region far from the diffusion surface. Therefore, it is difficult to exert an exchange-bonding action. At the same time, since the concentration of diffused elements is high in the region near the diffusion surface, heavy rare earths permeate the grain boundaries of the main phase, and the residual magnetism is significantly reduced. Further, as the heavy rare earth element wears faster and becomes deeper, the concentration of the heavy rare earth element decreases sharply, the component structure becomes non-uniform, and the performance improvement is hindered.
本発明は、上記した従来技術が有する問題を解決し、最適なミクロ構造を有するＮｄ－Ｆｅ－Ｂ系焼結磁性体の新たな製造方法を提供することを目的とする。 An object of the present invention is to solve the above-mentioned problems of the prior art and to provide a new method for producing an Nd-Fe-B-based sintered magnetic material having an optimum microstructure.
上記目的を達成するため、本願発明は、Ｎｄ－Ｆｅ－Ｂ系焼結磁性体の製造方法であって、
工程１：真空誘導炉を用いて多成分合金インゴットを製造し、続いて真空ストリップキャスト炉を用いて多成分合金ストリップを製造し、
前記多成分合金の原子比化学式はＰｒａＲＨｂＧａｃＣｕｄで示され、ＰｒはＰｒ元素、ＲＨはジスプロシウム元素又はテルビウム元素の少なくとも一つ、Ｇａはガリウム元素、Ｃｕは銅元素であり、
ａ、ｂ、ｃ、及びｄは、０．３０≦（ａ＋ｂ）／（ａ＋ｂ＋ｃ＋ｄ）≦０．６５、０．２０≦ｄ／（ｃ＋ｄ）≦０．５０、０．２３≦ｂ／（ａ＋ｂ）≦０．６０の関係式を満たし、
工程２：前記多成分合金ストリップを粉砕して粉末にし、前記Ｎｄ－Ｆｅ－Ｂ系焼結磁性体の表面に付着させ、
工程３：前記多成分合金粉末を付着させた前記Ｎｄ－Ｆｅ－Ｂ系焼結磁性体を高温拡散処理及び低温時効処理し、拡散処理後の前記Ｎｄ－Ｆｅ－Ｂ系焼結磁性体を得る、
ことを特徴とする。
In order to achieve the above object, the present invention is a method for producing an Nd—Fe—B-based sintered magnetic material.
Step 1: A vacuum induction furnace is used to make a multi-component alloy ingot, followed by a vacuum strip cast furnace to make a multi-component alloy strip.
The atomic specific chemical formula of the multi-component alloy is represented by Pr a RH b Ga c Cu d , where Pr is an Pr element, RH is at least one of a dysprosium element or a terbium element, Ga is a gallium element, and Cu is a copper element.
a, b, c, and d are 0.30 ≦ (a + b) / (a + b + c + d) ≦ 0.65, 0.20 ≦ d / (c + d) ≦ 0.50, 0.23 ≦ b / (a + b) ≦ Satisfy the relational expression of 0.60,
Step 2: The multi-component alloy strip is crushed into powder and adhered to the surface of the Nd-Fe-B-based sintered magnetic material.
Step 3: The Nd-Fe-B-based sintered magnetic material to which the multi-component alloy powder is attached is subjected to high-temperature diffusion treatment and low-temperature aging treatment to obtain the Nd-Fe-B-based sintered magnetic material after the diffusion treatment. ,
It is characterized by that.
また、前記多成分合金ストリップを粉砕した前記粉末の平均粒径は、１０μｍ～１０００μｍであり、より好ましくは、５０μｍ～６００μｍである、ことを特徴とする。 Further, the average particle size of the powder obtained by crushing the multi-component alloy strip is 10 μm to 1000 μm, more preferably 50 μm to 600 μm.
また、前記Ｎｄ－Ｆｅ－Ｂ系焼結磁性体の前記表面とは、配向方向に垂直な面である、ことを特徴とする Further, the surface of the Nd—Fe—B-based sintered magnetic material is a plane perpendicular to the orientation direction.
また、前記高温拡散処理の温度は７２０℃～９８０℃、拡散時間は５～２５時間であり、前記低温時効処理の温度は４８０℃～６８０℃、処理時間は１～１０時間である、ことを特徴とする。 Further, the temperature of the high temperature diffusion treatment is 720 ° C. to 980 ° C., the diffusion time is 5 to 25 hours, the temperature of the low temperature aging treatment is 480 ° C. to 680 ° C., and the treatment time is 1 to 10 hours. It is a feature.
また、拡散によって主相粒子の外周に導入されたテルビウム元素及び／又はジスプロシウム元素の分布領域は、いずれも拡散によって導入されたＰｒ元素の分布領域の範囲内である、ことを特徴とする。 Further, the distribution regions of the terbium element and / or the dysprosium element introduced to the outer periphery of the main phase particles by diffusion are both within the distribution region of the Pr element introduced by diffusion.
また、拡散によって導入されたテルビウム及び／又はジスプロシウム元素の磁性体内における分布深さは、少なくとも４００μｍである、ことを特徴とする。 Further, the distribution depth of the terbium and / or the dysprosium element introduced by diffusion in the magnetic body is at least 400 μm.
本願発明は、元素比を最適化した多成分低融点合金を製造し、それを粉末へと粉砕して拡散源とし、効果的に拡散する温度範囲を拡大し、湿潤性に優れるＰｒ、銅、ガリウム等の元素を用いることで、磁性体のより内部まで拡散させ易くなり、重希土類元素の拡散深さも向上することから、分布がより均一になる。 According to the present invention, a multi-component low melting point alloy having an optimized element ratio is produced, which is pulverized into a powder to be used as a diffusion source, the temperature range for effective diffusion is expanded, and Pr, copper, which has excellent wettability, is used. By using an element such as gallium, it becomes easier to diffuse into the inside of the magnetic material, and the diffusion depth of the heavy rare earth element is also improved, so that the distribution becomes more uniform.
また本願発明は、拡散合金の粒径を調整し、且つＮｄ－Ｆｅ－Ｂ系焼結磁性体の付着面を配向方向の面に垂直な面とし、拡散効率及び効果を更に向上させる。最終的に得られた磁性体では、拡散によって導入された重希土類元素が、拡散したＰｒ元素に付着して、主相粒子の外周に分布してシェル構造を形成する。主相粒子の中心領域に重希土類元素が入り込むことがないため、磁性体の残留磁気が大幅に低下することなく、Ｎｄ－Ｆｅ－Ｂ系焼結磁性体の保磁力を大幅に向上させることができる。 Further, in the present invention, the particle size of the diffusion alloy is adjusted, and the adhesion surface of the Nd—Fe—B-based sintered magnetic material is set to be a surface perpendicular to the surface in the orientation direction, further improving the diffusion efficiency and effect. In the finally obtained magnetic material, the heavy rare earth element introduced by diffusion adheres to the diffused Pr element and is distributed on the outer periphery of the main phase particles to form a shell structure. Since heavy rare earth elements do not enter the central region of the main phase particles, the coercive force of the Nd-Fe-B-based sintered magnetic material can be significantly improved without significantly reducing the residual magnetism of the magnetic material. can.
従来技術と対比した本発明の新規性及び進歩性は、上記のとおり多成分合金を用いてＮｄ－Ｆｅ－Ｂ系焼結磁性体に対して拡散を行う点にあるが、Ｐｒ、Ｃｕ、Ｇａ元素は融点が低く、低温であっても磁性体に浸透させることができ、且つ優れた拡散深さを備える。これが優先的に結晶粒界やコーナー部に入り込み、その後の重希土類元素の浸透が比較的容易になる。つまり、浸透速度が速く、深さが深くなる。本願発明は、拡散合金の粒径を調整し、且つＮｄ－Ｆｅ－Ｂ系焼結磁性体の付着面を配向方向の面に垂直な面とすることで、拡散効率と効果を更に向上させることができる。 The novelty and inventive step of the present invention in comparison with the prior art lies in the fact that the Nd—Fe—B-based sintered magnetic material is diffused by using a multi-component alloy as described above, but Pr, Cu, and Ga Elements have a low melting point, can penetrate magnetic materials even at low temperatures, and have an excellent diffusion depth. This preferentially enters the grain boundaries and corners, and the subsequent permeation of heavy rare earth elements becomes relatively easy. That is, the penetration rate is high and the depth is deep. INDUSTRIAL APPLICABILITY The present invention further improves the diffusion efficiency and effect by adjusting the particle size of the diffusion alloy and making the adhesion surface of the Nd-Fe-B-based sintered magnetic material a surface perpendicular to the plane in the orientation direction. Can be done.
より良好な理解と実施のため、以下、具体的実施例に基づいて本発明を詳細に説明する。 Hereinafter, the present invention will be described in detail based on specific examples for better understanding and implementation.
本願発明の基本構成は、概略以下のとおりである。
まず、原子比化学式ＰｒａＲＨｂＧａｃＣｕｄに基づいて原材料を配合する。ＰｒはＰｒ元素、ＲＨはジスプロシウム元素又はテルビウム元素の少なくとも一つ、Ｇａはガリウム元素、Ｃｕは銅元素である。ａ、ｂ、ｃ、及びｄは、０．３０≦（ａ＋ｂ）／（ａ＋ｂ＋ｃ＋ｄ）≦０．６５、０．２０≦ｄ／（ｃ＋ｄ）≦０．５０、０．２３≦ｂ／（ａ＋ｂ）≦０．６０の関係式を満たす。
The basic configuration of the present invention is as follows.
First, the raw materials are blended based on the atomic ratio chemical formula Pra a RH b Ga c Cu d . Pr is an Pr element, RH is at least one of a dysprosium element or a terbium element, Ga is a gallium element, and Cu is a copper element. a, b, c, and d are 0.30 ≦ (a + b) / (a + b + c + d) ≦ 0.65, 0.20 ≦ d / (c + d) ≦ 0.50, 0.23 ≦ b / (a + b) ≦ Satisfy the relational expression of 0.60.
上記の原材料をもとにして、真空誘導炉を用いて多成分合金インゴットを製造する。得られたインゴットを、真空ストリップキャスト炉を用いて多成分合金ストリップへと加工する。このストリップを平均粒径１０μｍ～１０００μｍ、好ましくは平均粒径５０μｍ～６００μｍの粉末へと粉砕し、素地重量比で２．０％の粉末を従来の設備とプロセスで製造したＮｄ－Ｆｅ－Ｂ系焼結磁性体の表面に付着させる。 Based on the above raw materials, a multi-component alloy ingot is manufactured using a vacuum induction furnace. The obtained ingot is processed into a multi-component alloy strip using a vacuum strip casting furnace. This strip is pulverized into a powder having an average particle size of 10 μm to 1000 μm, preferably an average particle size of 50 μm to 600 μm, and a powder having a base weight ratio of 2.0% is produced by a conventional facility and process. Adhere to the surface of the sintered magnetic material.
真空加熱炉を用いて拡散源粉末が付着した磁性体を熱処理する。高温拡散処理の温度は７２０℃～９８０℃、拡散時間は５～２５時間であり、低温時効処理の温度は４８０℃～６８０℃、処理時間は１～１０時間である。 A vacuum heating furnace is used to heat-treat the magnetic material to which the diffusion source powder is attached. The temperature of the high temperature diffusion treatment is 720 ° C. to 980 ° C., the diffusion time is 5 to 25 hours, the temperature of the low temperature aging treatment is 480 ° C. to 680 ° C., and the treatment time is 1 to 10 hours.
実施例１
原子比化学式Ｐｒ５０Ｔｂ１５Ｃｕ７Ｇａ２８に基づいて原材料を配合し、真空誘導炉を用いてインゴットを溶錬し、得られたインゴットを、真空ストリップキャスト炉を用いてストリップへと加工した。このストリップを平均粒径１０００μｍの粉末へと粉砕し、素地重量比で２．０％の粉末を従来の設備とプロセスで製造したＮｄ－Ｆｅ－Ｂ系焼結磁性体素地の表面へ付着させた。
Example 1
Raw materials were blended based on the atomic ratio chemical formula Pr 50 Tb 15 Cu 7 Ga 28 , the ingot was smelted using a vacuum induction furnace, and the obtained ingot was processed into strips using a vacuum strip cast furnace. This strip was crushed into a powder having an average particle size of 1000 μm, and a powder having a weight ratio of the base material of 2.0% was adhered to the surface of the Nd-Fe-B-based sintered magnetic material base material manufactured by the conventional equipment and process. ..
Ｎｄ－Ｆｅ－Ｂ系焼結磁性体サンプルの拡散方向の厚さは４．０ｍｍであり、通常成分のＮ５５規格の磁性体を選択し、初期性能は、Ｂｒ＝１５．０５ｋＧｓ、Ｈｃｊ＝９．５０ｋＯｅ、角形比Ｈｋ/Ｈｃｊ＝０．９５である。素地にはＮｄ、Ｆｅ、Ｂ、Ｃｕ、Ｃｏ等の元素を含む。 The thickness of the Nd-Fe-B-based sintered magnetic material sample in the diffusion direction is 4.0 mm, a magnetic material of N55 standard as a normal component is selected, and the initial performance is Br = 15.05 kGs, Hcj = 9. It is 50 kOe and the square ratio is Hk / Hcj = 0.95. The substrate contains elements such as Nd, Fe, B, Cu, and Co.
真空加熱炉を用いて拡散源粉末が付着した磁性体を熱処理した。高温拡散処理の温度は７２０℃、拡散時間は２５時間であり、低温時効処理の温度は４８０℃、処理時間は１０時間であった。 The magnetic material to which the diffusion source powder was attached was heat-treated using a vacuum heating furnace. The temperature of the high temperature diffusion treatment was 720 ° C., the diffusion time was 25 hours, the temperature of the low temperature aging treatment was 480 ° C., and the treatment time was 10 hours.
拡散完成後のサンプルの磁気特性に関する測定試験を行い、且つＥＤＳ（エネルギー分散型Ｘ線分光法）を用いて、拡散表面から４００～４１１μｍ離れた領域における元素分布を測定した。図１－１は、実施例１で製造したサンプルのＴｂ元素のＥＤＳ撮影分布写真であり、図１－２は実施例１で製造したサンプルのＰｒ元素のＥＤＳ撮影分布写真である。なお、図７は、当該ＥＤＳで撮影した磁性体表面の場所Ｘを示しており、図１～図６の全てにおいて共通している。 A measurement test was performed on the magnetic properties of the sample after the diffusion was completed, and the element distribution in a region 400 to 411 μm away from the diffusion surface was measured using EDS (energy dispersive X-ray spectroscopy). FIG. 1-1 is an EDS photographed distribution photograph of the Tb element of the sample produced in Example 1, and FIG. 1-2 is an EDS photographed distribution photograph of the Pr element of the sample produced in Example 1. Note that FIG. 7 shows the location X of the magnetic material surface photographed by the EDS, which is common to all of FIGS. 1 to 6.
図１－１、１－２から明らかなとおり、Ｔｂ元素の拡散深さは４００μｍを超えており、Ｐｒ元素とＴｂ元素は主相粒子の外周においてシェル構造を形成し、Ｔｂ元素の分布範囲はＰｒ元素の分布範囲を超えていないことが分かる。 As is clear from FIGS. 1-1 and 2, the diffusion depth of the Tb element exceeds 400 μm, the Pr element and the Tb element form a shell structure on the outer periphery of the main phase particles, and the distribution range of the Tb element is wide. It can be seen that the distribution range of Pr elements is not exceeded.
実施例２
原子比化学式Ｐｒ１２Ｔｂ１８Ｃｕ３５Ｇａ３５に基づいて原材料を配合し、真空誘導炉を用いてインゴットを溶錬し、得られたインゴットを、真空ストリップキャスト炉を用いてストリップへと加工した。このストリップを平均粒径１０μｍの粉末へと粉砕し、素地重量比で２．０％の粉末を従来の設備とプロセスで製造したＮｄ－Ｆｅ－Ｂ系焼結磁性体素地の表面へ付着させた。
Example 2
Raw materials were blended based on the atomic ratio chemical formula Pr 12 Tb 18 Cu 35 Ga 35 , the ingot was smelted using a vacuum induction furnace, and the obtained ingot was processed into strips using a vacuum strip cast furnace. This strip was crushed into a powder having an average particle size of 10 μm, and a powder having a weight ratio of the base material of 2.0% was adhered to the surface of the Nd-Fe-B-based sintered magnetic material base material manufactured by the conventional equipment and process. ..
Ｎｄ－Ｆｅ－Ｂ系焼結磁性体サンプルの拡散方向の厚さは４．０ｍｍであり、通常成分のＮ５５規格の磁性体を選択し、初期性能は、Ｂｒ＝１５．０５ｋＧｓ、Ｈｃｊ＝９．５０ｋＯｅ、角形比Ｈｋ/Ｈｃｊ＝０．９５である。素地にはＮｄ、Ｆｅ、Ｂ、Ｃｕ、Ｃｏ等の元素を含む。 The thickness of the Nd-Fe-B-based sintered magnetic material sample in the diffusion direction is 4.0 mm, a magnetic material of N55 standard as a normal component is selected, and the initial performance is Br = 15.05 kGs, Hcj = 9. It is 50 kOe and the square ratio is Hk / Hcj = 0.95. The substrate contains elements such as Nd, Fe, B, Cu, and Co.
真空加熱炉を用いて拡散源粉末が付着した磁性体を熱処理した。高温拡散処理の温度は９８０℃、拡散時間は５時間であり、低温時効処理の温度は６８０℃、処理時間は１時間であった。 The magnetic material to which the diffusion source powder was attached was heat-treated using a vacuum heating furnace. The temperature of the high temperature diffusion treatment was 980 ° C., the diffusion time was 5 hours, the temperature of the low temperature aging treatment was 680 ° C., and the treatment time was 1 hour.
拡散完成後のサンプルの磁気特性に関する測定試験を行い、且つＥＤＳ（エネルギー分散型Ｘ線分光法）を用いて、拡散表面から４００～４１１μｍ離れた領域における元素分布を測定した。図２－１は、実施例２で製造したサンプルのＴｂ元素のＥＤＳ撮影分布写真であり、図２－２は実施例２で製造したサンプルのＰｒ元素のＥＤＳ撮影分布写真である。 A measurement test on the magnetic properties of the sample after the completion of diffusion was carried out, and the element distribution in a region 400 to 411 μm away from the diffusion surface was measured using EDS (energy dispersive X-ray spectroscopy). FIG. 2-1 is an EDS photographed distribution photograph of the Tb element of the sample produced in Example 2, and FIG. 2-2 is an EDS photographed distribution photograph of the Pr element of the sample produced in Example 2.
図２－１、２－２から明らかなとおり、Ｔｂ元素の拡散深さは４００μｍを超えており、Ｐｒ元素とＴｂ元素は主相粒子の外周においてシェル構造を形成し、Ｔｂ元素の分布範囲はＰｒ元素の分布範囲を超えていないことが分かる。 As is clear from FIGS. 2-1 and 2-2, the diffusion depth of the Tb element exceeds 400 μm, the Pr element and the Tb element form a shell structure on the outer periphery of the main phase particles, and the distribution range of the Tb element is wide. It can be seen that the distribution range of Pr elements is not exceeded.
実施例３
原子比化学式Ｐｒ３０Ｔｂ２０Ｃｕ１５Ｇａ３５に基づいて原材料を配合し、真空誘導炉を用いてインゴットを溶錬し、得られたインゴットを、真空ストリップキャスト炉を用いてストリップへと加工した。このストリップを平均粒径５０μｍの粉末へと粉砕し、素地重量比で２．０％の粉末を従来の設備とプロセスで製造したＮｄ－Ｆｅ－Ｂ系焼結磁性体素地の表面へ付着させた。
Example 3
Raw materials were blended based on the atomic ratio chemical formula Pr 30 Tb 20 Cu 15 Ga 35 , the ingot was smelted using a vacuum induction furnace, and the obtained ingot was processed into strips using a vacuum strip cast furnace. This strip was crushed into a powder having an average particle size of 50 μm, and a powder having a weight ratio of the base material of 2.0% was adhered to the surface of the Nd-Fe-B-based sintered magnetic material base material manufactured by the conventional equipment and process. ..
Ｎｄ－Ｆｅ－Ｂ系焼結磁性体サンプルの拡散方向の厚さは４．０ｍｍであり、通常成分のＮ５５規格の磁性体を選択し、初期性能は、Ｂｒ＝１５．０５ｋＧｓ、Ｈｃｊ＝９．５０ｋＯｅ、角形比Ｈｋ/Ｈｃｊ＝０．９５である。素地にはＮｄ、Ｆｅ、Ｂ、Ｃｕ、Ｃｏ等の元素を含む。 The thickness of the Nd-Fe-B-based sintered magnetic material sample in the diffusion direction is 4.0 mm, a magnetic material of N55 standard as a normal component is selected, and the initial performance is Br = 15.05 kGs, Hcj = 9. It is 50 kOe and the square ratio is Hk / Hcj = 0.95. The substrate contains elements such as Nd, Fe, B, Cu, and Co.
真空加熱炉を用いて拡散源粉末が付着した磁性体を熱処理した。高温拡散処理の温度は９００℃、拡散時間は１０時間であり、低温時効処理の温度は５２０℃、処理時間は３時間であった。 The magnetic material to which the diffusion source powder was attached was heat-treated using a vacuum heating furnace. The temperature of the high temperature diffusion treatment was 900 ° C., the diffusion time was 10 hours, the temperature of the low temperature aging treatment was 520 ° C., and the treatment time was 3 hours.
拡散完成後のサンプルの磁気特性に関する測定試験を行い、且つＥＤＳ（エネルギー分散型Ｘ線分光法）を用いて、拡散表面から４００～４１１μｍ離れた領域における元素分布を測定した。図３－１は実施例３で製造したサンプルのＴｂ元素のＥＤＳ撮影分布写真であり、図３－２は実施例３で製造したサンプルのＰｒ元素のＥＤＳ撮影分布写真である。 A measurement test on the magnetic properties of the sample after the completion of diffusion was carried out, and the element distribution in a region 400 to 411 μm away from the diffusion surface was measured using EDS (energy dispersive X-ray spectroscopy). FIG. 3-1 is an EDS photographed distribution photograph of the Tb element of the sample produced in Example 3, and FIG. 3-2 is an EDS photographed distribution photograph of the Pr element of the sample produced in Example 3.
図３－１、３－２から明らかなとおり、Ｔｂ元素の拡散深さは４００μｍを超えており、Ｐｒ元素とＴｂ元素は主相粒子の外周においてシェル構造を形成し、Ｔｂ元素の分布範囲はＰｒ元素の分布範囲を超えていないことが分かる。 As is clear from FIGS. 3-1 and 3-2, the diffusion depth of the Tb element exceeds 400 μm, the Pr element and the Tb element form a shell structure on the outer periphery of the main phase particles, and the distribution range of the Tb element is wide. It can be seen that the distribution range of Pr elements is not exceeded.
実施例４
原子比化学式Ｐｒ３０Ｄｙ２０Ｃｕ１５Ｇａ３５に基づいて原材料を配合し、真空誘導炉を用いてインゴットを溶錬し、得られたインゴットを、真空ストリップキャスト炉を用いてストリップへと加工した。このストリップを平均粒径６００μｍの粉末へと粉砕し、素地重量比で２．０％の粉末を従来の設備とプロセスで製造したＮｄ－Ｆｅ－Ｂ系焼結磁性体素地の表面へ付着させた。
Example 4
Raw materials were blended based on the atomic ratio chemical formula Pr 30 Dy 20 Cu 15 Ga 35 , the ingot was smelted using a vacuum induction furnace, and the obtained ingot was processed into strips using a vacuum strip cast furnace. This strip was crushed into a powder having an average particle size of 600 μm, and a powder having a weight ratio of 2.0% was adhered to the surface of an Nd-Fe-B-based sintered magnetic substrate manufactured by conventional equipment and a process. ..
Ｎｄ－Ｆｅ－Ｂ系焼結磁性体サンプルの拡散方向の厚さは４．０ｍｍであり、通常成分のＮ５５規格の磁性体を選択し、初期性能は、Ｂｒ＝１５．０５ｋＧｓ、Ｈｃｊ＝９．５０ｋＯｅ、角形比Ｈｋ/Ｈｃｊ＝０．９５である。素地にはＮｄ、Ｆｅ、Ｂ、Ｃｕ、Ｃｏ等の元素を含む。 The thickness of the Nd-Fe-B-based sintered magnetic material sample in the diffusion direction is 4.0 mm, a magnetic material of N55 standard as a normal component is selected, and the initial performance is Br = 15.05 kGs, Hcj = 9. It is 50 kOe and the square ratio is Hk / Hcj = 0.95. The substrate contains elements such as Nd, Fe, B, Cu, and Co.
真空加熱炉を用いて拡散源粉末が付着した磁性体を熱処理した。高温拡散処理の温度は９００℃、拡散時間は１０時間であり、低温時効処理の温度は５２０℃、処理時間は３時間であった。 The magnetic material to which the diffusion source powder was attached was heat-treated using a vacuum heating furnace. The temperature of the high temperature diffusion treatment was 900 ° C., the diffusion time was 10 hours, the temperature of the low temperature aging treatment was 520 ° C., and the treatment time was 3 hours.
拡散完成後のサンプルの磁気特性に関する測定試験を行い、且つＥＤＳ（エネルギー分散型Ｘ線分光法）を用いて、拡散表面から４００～４１１μｍ離れた領域における元素分布を測定した。図４－１は、実施例４で製造したサンプルのＤｙ元素のＥＤＳ撮影分布写真であり、図４－２は実施例４で製造したサンプルのＰｒ元素のＥＤＳ撮影分布写真である。 A measurement test on the magnetic properties of the sample after the completion of diffusion was carried out, and the element distribution in a region 400 to 411 μm away from the diffusion surface was measured using EDS (energy dispersive X-ray spectroscopy). FIG. 4-1 is an EDS photographed distribution photograph of the Dy element of the sample produced in Example 4, and FIG. 4-2 is an EDS photographed distribution photograph of the Pr element of the sample produced in Example 4.
図４－１、４－２から明らかなとおり、Ｄｙ元素の拡散深さは４００μｍを超えており、Ｐｒ元素とＤｙ元素は主相粒子の外周においてシェル構造を形成し、Ｄｙ元素の分布範囲はＰｒ元素の分布範囲を超えていないことが分かる。 As is clear from FIGS. 4-1 and 4-2, the diffusion depth of the Dy element exceeds 400 μm, the Pr element and the Dy element form a shell structure on the outer periphery of the main phase particles, and the distribution range of the Dy element is wide. It can be seen that the distribution range of Pr elements is not exceeded.
実施例５
原子比化学式Ｐｒ３０Ｔｂ１０Ｄｙ１０Ｃｕ１５Ｇａ３５に基づいて原材料を配合し、真空誘導炉を用いてインゴットを溶錬し、得られたインゴットを、真空ストリップキャスト炉を用いてストリップへと加工した。ストリップを平均粒径３００μｍの粉末へと粉砕し、素地重量比で２．０％の粉末を従来の設備とプロセスで製造したＮｄ－Ｆｅ－Ｂ系焼結磁性体素地の表面へ付着させた。
Example 5
Raw materials are blended based on the atomic ratio chemical formula Pr 30 Tb 10 Dy 10 Cu 15 Ga 35 , the ingot is smelted using a vacuum induction furnace, and the obtained ingot is processed into strips using a vacuum strip cast furnace. did. The strip was pulverized into a powder having an average particle size of 300 μm, and a powder having a weight ratio of the substrate of 2.0% was adhered to the surface of the Nd—Fe—B-based sintered magnetic substrate produced by the conventional equipment and process.
Ｎｄ－Ｆｅ－Ｂ系焼結磁性体サンプルの拡散方向の厚さは４．０ｍｍであり、通常成分のＮ５５規格の磁性体を選択し、初期性能は、Ｂｒ＝１５．０５ｋＧｓ、Ｈｃｊ＝９．５０ｋＯｅ、角形比Ｈｋ/Ｈｃｊ＝０．９５であった。素地にはＮｄ、Ｆｅ、Ｂ、Ｃｕ、Ｃｏ等の元素を含む。 The thickness of the Nd-Fe-B-based sintered magnetic material sample in the diffusion direction is 4.0 mm, a magnetic material of N55 standard as a normal component is selected, and the initial performance is Br = 15.05 kGs, Hcj = 9. The square ratio was 50 kOe and the square ratio was Hk / Hcj = 0.95. The substrate contains elements such as Nd, Fe, B, Cu, and Co.
真空加熱炉を用いて拡散源粉末が付着した磁性体を熱処理した。高温拡散処理の温度は９００℃、拡散時間は１０時間であり、低温時効処理の温度は５２０℃、処理時間は３時間であった。 The magnetic material to which the diffusion source powder was attached was heat-treated using a vacuum heating furnace. The temperature of the high temperature diffusion treatment was 900 ° C., the diffusion time was 10 hours, the temperature of the low temperature aging treatment was 520 ° C., and the treatment time was 3 hours.
拡散完成後のサンプルの磁気特性に関する測定試験を行い、且つＥＤＳ（エネルギー分散型Ｘ線分光法）を用いて、拡散表面から４００～４１１μｍ離れた領域における元素分布を測定した。図５－１は実施例５で製造したサンプルのＴｂ＋Ｄｙ元素のＥＤＳ撮影分布写真であり、図５－２は実施例５で製造したサンプルのＰｒ元素のＥＤＳ撮影分布写真である。 A measurement test on the magnetic properties of the sample after the completion of diffusion was carried out, and the element distribution in a region 400 to 411 μm away from the diffusion surface was measured using EDS (energy dispersive X-ray spectroscopy). FIG. 5-1 is an EDS photographed distribution photograph of the Tb + Dy element of the sample produced in Example 5, and FIG. 5-2 is an EDS photographed distribution photograph of the Pr element of the sample produced in Example 5.
図５－１、５－２から明らかなとおり、Ｔｂ＋Ｄｙ元素の拡散深さは４００μｍを超えており、Ｐｒ元素とＴｂ＋Ｄｙ元素は主相粒子の外周においてシェル構造を形成し、Ｔｂ＋Ｄｙ元素の分布範囲はＰｒ元素の分布範囲を超えていないことが分かる。 As is clear from FIGS. 5-1 and 5-2, the diffusion depth of the Tb + Dy element exceeds 400 μm, the Pr element and the Tb + Dy element form a shell structure on the outer periphery of the main phase particles, and the distribution range of the Tb + Dy element is wide. It can be seen that the distribution range of Pr elements is not exceeded.
実施例における拡散源合金元素の比率及び拡散後のサンプルの磁気特性及び重希土類含有量を、表１と表２にそれぞれ示す。 The ratio of the diffusion source alloy elements in the examples, the magnetic properties of the sample after diffusion, and the heavy rare earth content are shown in Tables 1 and 2, respectively.
表１：実施例の拡散源合金元素の比率
表２：実施例の拡散後のサンプルの磁気特性及び重希土類含有量
比較例１
原子比化学式Ｐｒ１Ｔｂ６９Ｃｕ２９Ｇａ１に基づいて原材料を配合し、真空誘導炉を用いてインゴットを溶錬し、得られたインゴットを、真空ストリップキャスト炉を用いてストリップへと加工した。このストリップを平均粒径３００μｍの粉末へと粉砕し、素地重量比で２．０％の粉末を従来の設備とプロセスで製造したＮｄ－Ｆｅ－Ｂ系焼結磁性体素地の表面へ付着させた。
Comparative Example 1
Raw materials were blended based on the atomic ratio chemical formula Pr 1 Tb 69 Cu 29 Ga 1 , the ingot was smelted using a vacuum induction furnace, and the obtained ingot was processed into strips using a vacuum strip cast furnace. This strip was crushed into a powder having an average particle size of 300 μm, and a powder having a weight ratio of 2.0% was adhered to the surface of an Nd-Fe-B-based sintered magnetic substrate manufactured by conventional equipment and a process. ..
Ｎｄ－Ｆｅ－Ｂ系焼結磁性体サンプルの拡散方向の厚さは４．０ｍｍであり、通常成分のＮ５５規格の磁性体を選択し、初期性能は、Ｂｒ＝１５．０５ｋＧｓ、Ｈｃｊ＝９．５０ｋＯｅ、角形比Ｈｋ/Ｈｃｊ＝０．９５である。素地にはＮｄ、Ｆｅ、Ｂ、Ｃｕ、Ｃｏ等の元素を含む。 The thickness of the Nd-Fe-B-based sintered magnetic material sample in the diffusion direction is 4.0 mm, a magnetic material of N55 standard as a normal component is selected, and the initial performance is Br = 15.05 kGs, Hcj = 9. It is 50 kOe and the square ratio is Hk / Hcj = 0.95. The substrate contains elements such as Nd, Fe, B, Cu, and Co.
真空加熱炉を用いて拡散源粉末が付着した磁性体を熱処理した。高温拡散処理の温度は９００℃、拡散時間は１０時間であり、低温時効処理の温度は５２０℃、処理時間は３時間であった。拡散完成後のサンプルの磁気特性に関する測定試験を行った。 The magnetic material to which the diffusion source powder was attached was heat-treated using a vacuum heating furnace. The temperature of the high temperature diffusion treatment was 900 ° C., the diffusion time was 10 hours, the temperature of the low temperature aging treatment was 520 ° C., and the treatment time was 3 hours. A measurement test was conducted on the magnetic properties of the sample after the diffusion was completed.
比較例２
原子比化学式Ｐｒ６９Ｔｂ１Ｃｕ１０Ｇａ２０に基づいて原材料を配合し、真空誘導炉を用いてインゴットを溶錬し、得られたインゴットを、真空ストリップキャスト炉を用いてストリップへと加工した。このストリップを平均粒径３００μｍの粉末へと粉砕し、素地重量比で２．０％の粉末を従来の設備とプロセスで製造したＮｄ－Ｆｅ－Ｂ系焼結磁性体素地の表面へ付着させた。
Comparative Example 2
Raw materials were blended based on the atomic ratio chemical formula Pr 69 Tb 1 Cu 10 Ga 20 , the ingot was smelted using a vacuum induction furnace, and the obtained ingot was processed into strips using a vacuum strip cast furnace. This strip was crushed into a powder having an average particle size of 300 μm, and a powder having a weight ratio of 2.0% was adhered to the surface of an Nd-Fe-B-based sintered magnetic substrate manufactured by conventional equipment and a process. ..
Ｎｄ－Ｆｅ－Ｂ系焼結磁性体サンプルの拡散方向の厚さは４．０ｍｍであり、通常成分のＮ５５規格の磁性体を選択し、初期性能は、Ｂｒ＝１５．０５ｋＧｓ、Ｈｃｊ＝９．５０ｋＯｅ、角形比Ｈｋ/Ｈｃｊ＝０．９５である。素地にはＮｄ、Ｆｅ、Ｂ、Ｃｕ、Ｃｏ等の元素を含む。 The thickness of the Nd-Fe-B-based sintered magnetic material sample in the diffusion direction is 4.0 mm, a magnetic material of N55 standard as a normal component is selected, and the initial performance is Br = 15.05 kGs, Hcj = 9. It is 50 kOe and the square ratio is Hk / Hcj = 0.95. The substrate contains elements such as Nd, Fe, B, Cu, and Co.
真空加熱炉を用いて拡散源粉末が付着した磁性体を熱処理した。高温拡散処理の温度は９００℃、拡散時間は１０時間であり、低温時効処理の温度は５２０℃、処理時間は３時間であった。拡散完成後のサンプルの磁気特性に関する測定試験を行った。 The magnetic material to which the diffusion source powder was attached was heat-treated using a vacuum heating furnace. The temperature of the high temperature diffusion treatment was 900 ° C., the diffusion time was 10 hours, the temperature of the low temperature aging treatment was 520 ° C., and the treatment time was 3 hours. A measurement test was conducted on the magnetic properties of the sample after the diffusion was completed.
比較例３
原子比化学式Ｐｒ２０Ｔｂ５Ｃｕ４０Ｇａ３５に基づいて原材料を配合し、真空誘導炉を用いてインゴットを溶錬し、得られたインゴットを、真空ストリップキャスト炉を用いてストリップへと加工した。このストリップを平均粒径３００μｍの粉末へと粉砕し、素地重量比で２．０％の粉末を従来の設備とプロセスで製造したＮｄ－Ｆｅ－Ｂ系焼結磁性体素地の表面へ付着させた。
Comparative Example 3
Raw materials were blended based on the atomic ratio chemical formula Pr 20 Tb 5 Cu 40 Ga 35 , the ingot was smelted using a vacuum induction furnace, and the obtained ingot was processed into strips using a vacuum strip cast furnace. This strip was crushed into a powder having an average particle size of 300 μm, and a powder having a weight ratio of 2.0% was adhered to the surface of an Nd-Fe-B-based sintered magnetic substrate manufactured by conventional equipment and a process. ..
Ｎｄ－Ｆｅ－Ｂ系焼結磁性体サンプルの拡散方向の厚さは４．０ｍｍであり、通常成分のＮ５５規格の磁性体を選択し、初期性能は、Ｂｒ＝１５．０５ｋＧｓ、Ｈｃｊ＝９．５０ｋＯｅ、角形比Ｈｋ/Ｈｃｊ＝０．９５である。素地にはＮｄ、Ｆｅ、Ｂ、Ｃｕ、Ｃｏ等の元素を含む。 The thickness of the Nd-Fe-B-based sintered magnetic material sample in the diffusion direction is 4.0 mm, a magnetic material of N55 standard as a normal component is selected, and the initial performance is Br = 15.05 kGs, Hcj = 9. It is 50 kOe and the square ratio is Hk / Hcj = 0.95. The substrate contains elements such as Nd, Fe, B, Cu, and Co.
真空加熱炉を用いて拡散源粉末が付着した磁性体を熱処理した。高温拡散処理の温度は９００℃、拡散時間は１０時間であり、低温時効処理の温度は５２０℃、処理時間は３時間であった。 The magnetic material to which the diffusion source powder was attached was heat-treated using a vacuum heating furnace. The temperature of the high temperature diffusion treatment was 900 ° C., the diffusion time was 10 hours, the temperature of the low temperature aging treatment was 520 ° C., and the treatment time was 3 hours.
拡散完成後のサンプルの磁気特性に関する測定試験を行い、且つＥＤＳ（エネルギー分散型Ｘ線分光法）を用いて、拡散表面から４００～４１１μｍ離れた領域における元素分布を測定した。図６－１は比較例３で製造したサンプルのＴｂ元素のＥＤＳ撮影分布写真であり、図６－２は比較例３で製造したサンプルのＰｒ元素のＥＤＳ撮影分布写真である。 A measurement test on the magnetic properties of the sample after the completion of diffusion was carried out, and the element distribution in a region 400 to 411 μm away from the diffusion surface was measured using EDS (energy dispersive X-ray spectroscopy). FIG. 6-1 is an EDS photographed distribution photograph of the Tb element of the sample produced in Comparative Example 3, and FIG. 6-2 is an EDS photographed distribution photograph of the Pr element of the sample produced in Comparative Example 3.
図６－１、図６－２から明らかなとおり、４００μｍ以下の深さではＴｂ元素の分布を検測することができず、検測できるのはＰｒ元素の分布のみである。 As is clear from FIGS. 6-1 and 6-2, the distribution of the Tb element cannot be inspected at a depth of 400 μm or less, and only the distribution of the Pr element can be inspected.
比較例の拡散源合金元素の比率及び拡散後のサンプルの磁気特性及び重希土類含有量を、表３と表４にそれぞれ示す。 Tables 3 and 4 show the ratio of the diffusion source alloy elements of the comparative example, the magnetic properties of the sample after diffusion, and the heavy rare earth content, respectively.
表３：比較例の拡散源合金元素の比率
表４：比較例の拡散後のサンプルの磁気特性及び重希土類含有量
実施例１～実施例５の結果から、重希土類の浸透量が０．６２重量％を超えない条件において、拡散後の保磁力増加値はいずれも８．８５ｋＯｅ以上であり、且つ拡散後の残留磁気量は１４．７５ｋＧｓ以上であること、即ち、重希土類の使用量が少なくとも、保磁力の大幅な向上を実現し、且つ残留磁気が顕著に低下していないことが分かる。 From the results of Examples 1 to 5, the increase value of the coercive force after diffusion is 8.85 kOe or more under the condition that the permeation amount of the heavy rare earth does not exceed 0.62% by weight, and the residual magnetic charge after diffusion is obtained. It can be seen that the amount of magnetism is 14.75 kGs or more, that is, the amount of heavy rare earth used is at least a significant improvement in coercive force, and the residual magnetism is not significantly reduced.
また上記のとおり、ＥＤＳ（エネルギー分散型Ｘ線分光法）を用いて、拡散表面から４００～４１１μｍ離れた深さ領域における元素分布を測定した結果、重希土類元素の拡散深さはいずれも４００μｍを超え、Ｐｒ元素と重希土類元素は主相粒子の外周においてシェル構造を形成し、重希土類元素の分布範囲はＰｒ元素の分布範囲を超えていないことが分かる。 As described above, as a result of measuring the element distribution in the depth region 400 to 411 μm away from the diffusion surface using EDS (energy dispersion type X-ray spectroscopy), the diffusion depth of all heavy rare earth elements was 400 μm. It can be seen that the Pr element and the heavy rare earth element form a shell structure on the outer periphery of the main phase particles, and the distribution range of the heavy rare earth element does not exceed the distribution range of the Pr element.
この構造は、主相粒子間の結晶磁気異方性場を増加させ、磁性体の保磁力を向上させるだけでなく、重希土類元素が主相粒子の中心に入り込むことによって引き起こされる残留磁気の大幅な減少を回避することができる。 This structure not only increases the magnetocrystalline anisotropy field between the main phase particles and improves the coercive force of the magnetic material, but also significantly the residual magnetism caused by the heavy rare earth elements entering the center of the main phase particles. It is possible to avoid such a decrease.
比較例１では、Ｐｒ１Ｔｂ６９Ｃｕ２９Ｇａ１合金を用いて拡散させたが、拡散後の保磁力は大幅に向上するものの、重希土類の浸透量が多く、重希土類の重量比が１．６８％、同時に残留磁気の低減値が０．８２ｋＧｓに達し、磁性体の総合性能は低く、コストパフォーマンスも悪い。 In Comparative Example 1, Pr 1 Tb 69 Cu 29 Ga 1 alloy was used for diffusion, and although the coercive force after diffusion was significantly improved, the amount of heavy rare earth permeation was large and the weight ratio of heavy rare earth was 1. 68%, at the same time, the reduction value of residual magnetism reaches 0.82 kGs, the overall performance of the magnetic material is low, and the cost performance is also poor.
また比較例２では、Ｐｒ６９Ｔｂ１Ｃｕ１０Ｇａ２０合金を拡散源として用いたが、低融点元素は拡散工程において各元素の拡散深さは深くなり、ミクロ構造も均一となるものの、拡散源中に添加される重希土類の量が少なすぎるため、拡散後の結晶粒界に、結晶磁気異方性場を大きく向上させる物質を形成できず、保磁力の増加も僅かであった。 Further, in Comparative Example 2, a Pr 69 Tb 1 Cu 10 Ga 20 alloy was used as a diffusion source. However, although the low melting point element has a deep diffusion depth and a uniform microstructure in the diffusion step, it is a diffusion source. Since the amount of heavy rare earth added therein was too small, a substance that greatly improved the crystal magnetic anisotropic field could not be formed at the grain boundaries after diffusion, and the increase in coercive force was slight.
さらに比較例３では、各実施例と類似するＰｒ－Ｔｂ－Ｃｕ－Ｇａの４成分合金を拡散源として用いたが、合金成分に占めるＰｒとＴｂの比率がやや低く、元素濃度も低いことから、拡散の駆動エネルギーが減少してしまった。特に、ＥＤＳ撮影分布写真から明らかなとおり、深さ４００μｍ以降はＴｂ元素の分布が検出されなかった。これによって保磁力の向上が抑制されたものと推測される。 Further, in Comparative Example 3, a four-component alloy of Pr-Tb-Cu-Ga similar to each example was used as a diffusion source, but the ratio of Pr and Tb in the alloy components was slightly low, and the element concentration was also low. , The driving energy of diffusion has decreased. In particular, as is clear from the EDS photographed distribution photograph, the distribution of the Tb element was not detected after the depth of 400 μm. It is presumed that this suppressed the improvement of the coercive force.
上記の通り、本発明の方法によって製造されたＮｄ－Ｆｅ－Ｂ系焼結磁性体は、より高い磁気特性およびより良好なミクロ構造を有する。 As mentioned above, the Nd-Fe-B based sintered magnetic material produced by the method of the present invention has higher magnetic properties and better microstructure.
多成分合金を用いてＮｄ－Ｆｅ－Ｂ系焼結磁性体に対して拡散を行う本願発明によれば、Ｐｒ、Ｃｕ、Ｇａ元素は融点が低く、低温であっても磁性体に浸透させることができ、且つ優れた拡散深さを奏することができる。拡散合金の粒径が合理的な範囲内にあるためであり、これにより拡散面での分布が均一になるだけでなく、酸化が抑制され、効果が保証される。 According to the present invention in which diffusion is performed on an Nd—Fe—B-based sintered magnetic material using a multi-component alloy, the Pr, Cu, and Ga elements have a low melting point and are allowed to permeate the magnetic material even at a low temperature. And can produce an excellent diffusion depth. This is because the particle size of the diffusion alloy is within a reasonable range, which not only makes the distribution on the diffusion surface uniform, but also suppresses oxidation and guarantees the effect.
また、拡散源の付着面を配向方向の面に垂直な面とすることで、拡散温度に相当する温度下で、拡散合金の各元素は、配向方向に平行な方向に沿って素地内に入り込む。関連する研究によると、Ｎｄ－Ｆｅ－Ｂ系焼結磁性体の配向方向に平行な方向のミクロ構造には、より多くの結晶粒界相分布が存在する。Ｐｒ及び重希土類元素が浸透すると、一部が主相粒子の外周のＮｄ２Ｆｅ１４Ｂと置き換わり、元の主相粒子の外側に、より高い結晶磁気異方性場を有するＰｒ２Ｆｅ１４Ｂ及びＤｙ２Ｆｅ１４Ｂ／Ｔｂ２Ｆｅ１４Ｂシェル構造を形成し、磁性体の保磁力を大幅に改善することができる。 Further, by making the adhesion surface of the diffusion source a surface perpendicular to the plane in the orientation direction, each element of the diffusion alloy enters the substrate along the direction parallel to the orientation direction at a temperature corresponding to the diffusion temperature. .. According to a related study, there are more grain boundary phase distributions in the microstructure in the direction parallel to the orientation direction of the Nd-Fe-B based sintered magnetic material. When Pr and heavy rare earth elements permeate, part of it replaces Nd 2 Fe 14 B on the outer periphery of the main phase particles, and Pr 2 Fe 14 B has a higher crystalline magnetic anisotropy field outside the original main phase particles. And Dy 2 Fe 14 B / Tb 2 Fe 14 B shell structure can be formed, and the coercive force of the magnetic material can be significantly improved.
更に、Ｐｒ及びＤｙ／Ｔｂの置換は、磁性体の表面でのみ発生し、主相の結晶粒子の中心には浸透しないため、磁性体の残留磁気はさほど低下しない。Ｐｒの拡散能力はＤｙ／Ｔｂよりも強いことから、拡散温度が低い場合や拡散時間が短い場合であっても、Ｐｒ元素は結晶粒界まで効果的に拡散していく。主にＰｒ元素が先に入り込むと、主相粒子の外周にＰｒ２Ｆｅ１４Ｂが優先的に形成されるため、続いて拡散され浸透する重希土類元素は、主相粒子内部により深く拡散することが困難になり、シェル層は外周にのみ形成され、Ｈａが向上して保磁力が高まるだけでなく、Ｊｓの過度の減少による残留磁気の過度の減少が回避されるとともに、Ｃｕ及びＧａの浸透により、主相の結晶粒子間の磁気交換結合を抑制する作用も奏し、保磁力を更に高めることができる。 Further, since the substitution of Pr and Dy / Tb occurs only on the surface of the magnetic material and does not penetrate into the center of the crystal particles of the main phase, the residual magnetism of the magnetic material does not decrease so much. Since the diffusion ability of Pr is stronger than that of Dy / Tb, the Pr element effectively diffuses to the grain boundaries even when the diffusion temperature is low or the diffusion time is short. When the Pr element mainly enters first, Pr 2 Fe 14 B is preferentially formed on the outer periphery of the main phase particles, so that the heavy rare earth element that is subsequently diffused and permeates diffuses deeper inside the main phase particles. The shell layer is formed only on the outer periphery, and not only the Ha is improved and the coercive force is increased, but also the excessive decrease of the residual magnetism due to the excessive decrease of Js is avoided, and the penetration of Cu and Ga is prevented. As a result, it also has the effect of suppressing the magnetic exchange bond between the crystal particles of the main phase, and the coercive force can be further enhanced.
上記実施例は、本発明の具体的な実施方式の説明のみに供されるものであり、本発明を制限するものではない。本発明の内容及びロジックに行われるあらゆる補正、置換等はいずれも本発明の保護範囲内である。 The above-mentioned examples are provided only for the description of the specific embodiment of the present invention, and do not limit the present invention. All corrections, substitutions, etc. made to the content and logic of the present invention are within the scope of the present invention.
Claims (7)
工程１：真空誘導炉を用いて多成分合金インゴットを製造し、続いて真空ストリップキャスト炉を用いて多成分合金ストリップを製造し、
前記多成分合金の原子比化学式はＰｒａＲＨｂＧａｃＣｕｄで示され、ＰｒはＰｒ元素、ＲＨはジスプロシウム元素又はテルビウム元素の少なくとも一つ、Ｇａはガリウム元素、Ｃｕは銅元素であり、
ａ、ｂ、ｃ、及びｄは、０．３０≦（ａ＋ｂ）／（ａ＋ｂ＋ｃ＋ｄ）≦０．６５、０．２０≦ｄ／（ｃ＋ｄ）≦０．５０、０．２３≦ｂ／（ａ＋ｂ）≦０．６０の関係式を満たし、
工程２：前記多成分合金ストリップを粉砕して粉末にし、前記Ｎｄ－Ｆｅ－Ｂ系焼結磁性体の表面に付着させ、
工程３：前記多成分合金粉末を付着させた前記Ｎｄ－Ｆｅ－Ｂ系焼結磁性体を高温拡散処理及び低温時効処理し、拡散処理後の前記Ｎｄ－Ｆｅ－Ｂ系焼結磁性体を得る、
ことを特徴とするＮｄ－Ｆｅ－Ｂ系焼結磁性体の製造方法。 A method for producing an Nd-Fe-B-based sintered magnetic material.
Step 1: A vacuum induction furnace is used to make a multi-component alloy ingot, followed by a vacuum strip cast furnace to make a multi-component alloy strip.
The atomic specific chemical formula of the multi-component alloy is represented by Pr a RH b Ga c Cu d , where Pr is an Pr element, RH is at least one of a dysprosium element or a terbium element, Ga is a gallium element, and Cu is a copper element.
a, b, c, and d are 0.30 ≦ (a + b) / (a + b + c + d) ≦ 0.65, 0.20 ≦ d / (c + d) ≦ 0.50, 0.23 ≦ b / (a + b) ≦ Satisfy the relational expression of 0.60,
Step 2: The multi-component alloy strip is crushed into powder and adhered to the surface of the Nd-Fe-B-based sintered magnetic material.
Step 3: The Nd-Fe-B-based sintered magnetic material to which the multi-component alloy powder is attached is subjected to high-temperature diffusion treatment and low-temperature aging treatment to obtain the Nd-Fe-B-based sintered magnetic material after the diffusion treatment. ,
A method for producing an Nd-Fe-B-based sintered magnetic material, which is characterized by the above.
ことを特徴とする請求項１に記載のＮｄ－Ｆｅ－Ｂ系焼結磁性体の製造方法。 The average particle size of the powder obtained by crushing the multi-component alloy strip is 10 μm to 1000 μm.
The method for producing an Nd—Fe—B-based sintered magnetic material according to claim 1.
ことを特徴とする請求項１に記載のＮｄ－Ｆｅ－Ｂ系焼結磁性体の製造方法。 The average particle size of the powder obtained by crushing the multi-component alloy strip is 50 μm to 600 μm.
The method for producing an Nd—Fe—B-based sintered magnetic material according to claim 1.
ことを特徴とする請求項１ないし３のいずれか１項に記載のＮｄ－Ｆｅ－Ｂ系焼結磁性体の製造方法。 The surface of the Nd—Fe—B-based sintered magnetic material is a surface perpendicular to the orientation direction.
The method for producing an Nd—Fe—B-based sintered magnetic material according to any one of claims 1 to 3, wherein the Nd—Fe—B-based sintered magnetic material is produced.
前記低温時効処理の温度は４８０℃～６８０℃、処理時間は１～１０時間である、
ことを特徴とする請求項１ないし４のいずれか１項に記載のＮｄ－Ｆｅ－Ｂ系焼結磁性体の製造方法。 The temperature of the high temperature diffusion treatment is 720 ° C to 980 ° C, and the diffusion time is 5 to 25 hours.
The temperature of the low temperature aging treatment is 480 ° C to 680 ° C, and the treatment time is 1 to 10 hours.
The method for producing an Nd—Fe—B-based sintered magnetic material according to any one of claims 1 to 4, wherein the Nd—Fe—B-based sintered magnetic material is produced.
ことを特徴とする請求項１ないし５のいずれか１項に記載のＮｄ－Ｆｅ－Ｂ系磁性体の製造方法。 The distribution regions of the terbium element and / or the dysprosium element introduced to the outer periphery of the main phase particles by diffusion are both within the distribution region of the Pr element introduced by diffusion.
The method for producing an Nd—Fe—B-based magnetic material according to any one of claims 1 to 5, wherein the Nd—Fe—B-based magnetic material is produced.
ことを特徴とする請求項１ないし６のいずれか１項に記載のＮｄ－Ｆｅ－Ｂ系磁性体の製造方法。 The depth of distribution of the terbium and / or dysprosium element introduced by diffusion in the magnetic body is at least 400 μm.
The method for producing an Nd—Fe—B-based magnetic material according to any one of claims 1 to 6, wherein the Nd—Fe—B-based magnetic material is produced.
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